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I would like to know what methods would be suitable to determine if an alloy of 2 elements is a single phase or two phase alloy.

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    $\begingroup$ Microscopy (electron, optical). Diffraction (electron, x-ray). Various chemical techniques, often associated with microscopy. Any spatially-resolved analytical composition technique. $\endgroup$ – Jon Custer Jan 30 at 13:42
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The most suitable technique would be selected area electron diffraction SAED in an electron microscope. If there are two phases with distinct morphology, this will seen in the micrograph and then the SAED will confirm that there are two different crystallographic phases. Techniques using XRay probes will not work because the spot size is too large.

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